Methyl iodide → 1-Chloro-2-methoxy-3-methylbenzene

HRID 1042356ノート

反応式

HRID 1042356 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[OH:9].CI.[C:12]([O-])([O-])=O.[K+].[K+]>CC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[O:9][CH3:12]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 68982-Chloro-6-methylphenolHCID 11430Potassium Carbonate

生成物 1

HCID 134345771-Chloro-2-methoxy-3-methylbenzene

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

2-Chloro-6-methyl-phenol (12.00 g, 84.20 mmol) was mixed with MeI (10.50 mL, 0.17 mol) and K2CO3 (17.40 g, 0.13 mol) in acetone in acetone and the resulting reaction mixture was refluxed for 14 hours. The reaction mixture was cooled to room temperature, and then concentrated. The residue was diluted with Et2O. The resulting solution was washed with H2O (3×150 mL) and brine (1×200 mL), then dried over MgSO4 and concentrated. Purification by column chromatography using hex:EtOAc (4:1) as the eluant afforded the title compound.

後処理

  1. customthe resulting reaction mixture
  2. temperaturewas refluxed for 14 hours
  3. concentrationconcentrated
  4. additionThe residue was diluted with Et2O
  5. washThe resulting solution was washed with H2O (3×150 mL) and brine (1×200 mL)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated
  8. customPurification by column chromatography

出典と根拠

ORDレコード
ord-7988336ac1e94ff799bc3e16e2a1a0da
出典データセット
uspto-grants-2013_10
特許番号
US08557853B2

反応ノート

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